A ceramic silicone rubber self-adhesive material
By using ceramicized treatment and composite flame retardant in silicone rubber self-adhesive materials, the problem of insufficient flame retardant performance of existing materials is solved, and efficient flame retardant and fire-resistant performance is achieved, which is suitable for wire and cable connections in high-temperature environments.
Patent Information
- Application Number
- CN202410744565.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-11
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2044-06-11
AI Technical Summary
The existing silicone rubber self-adhesive materials have insufficient flame retardant performance during long-term use, which may lead to an increase in the temperature of the cable or cable, causing fires, and cannot effectively prevent the fire from spreading in high-temperature environments.
Using ceramic silicone rubber self-adhesive material, a composite flame retardant with a core-shell structure is prepared by combining kaolin with inorganic powders such as magnesium hydroxide, and flame retardant compounds such as diphenyl phosphine oxide and cispropylene phosphonic acid are added to the material to form a flame retardant layer with a three-dimensional network envelope structure.
The flame retardant and fire resistance of ceramic silicone rubber self-adhesive materials are significantly improved, while maintaining excellent bonding and mechanical properties, ensuring the quality and quality of the material.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of self-adhesive materials, and more specifically to a ceramic silicone rubber self-adhesive material. Background Art
[0002] Silicone rubber self-adhesive material is a commonly used connection material in power systems. It is mainly used for insulation, sealing and waterproofing of wire and cable joints. It can also be used for protection, repair and sealing of pipelines. During the manufacturing, storage, transportation and installation of wires and cables, the insulation of the cable core is easily scratched by external forces. During the connection of various wires and cables, the insulation of the core also needs to be stripped. After scratching and stripping, the insulation performance will be lost and the normal power supply function cannot be maintained. The existing technology often uses silicone rubber self-adhesive materials for repair.
[0003] The patent document with application number "CN201610863836.3" discloses a self-adhesive silicone rubber material and a preparation method thereof, which is characterized in that 100 parts of silicone rubber, 10 to 80 parts of a reinforcing agent, 1 to 9 parts of a controlling agent, and 0 to 5 parts of a sensitizer are mixed and molded, and then cross-linked by gamma-ray radiation with a radiation absorption dose of 30 to 100 kGy to obtain a self-adhesive silicone rubber material with excellent performance.
[0004] Although the self-adhesive silicone rubber material provided in the above patent document has excellent bonding properties, its flame retardant properties are relatively insufficient. When used for a long time, it may cause the temperature of the cable or cable to rise, which may easily cause a fire. Furthermore, some special application scenarios have higher performance requirements for self-adhesive tapes. For example, in high temperature environments such as fires, it is necessary to have excellent flame retardant properties to prevent the spread of fire.
[0005] Therefore, the present invention provides a ceramic silicone rubber self-adhesive material to solve this technical problem. Summary of the invention
[0006] The purpose of the present invention is to provide a ceramic silicone rubber self-adhesive material. The provided ceramic silicone rubber self-adhesive material not only has excellent bonding properties and mechanical properties, but also has excellent flame retardant properties, effectively ensuring the quality of the ceramic silicone rubber self-adhesive material.
[0007] To achieve the above object, the present invention provides the following technical solutions:
[0008] A ceramic silicone rubber self-adhesive material is composed of the following raw materials in parts by weight: 85-100 parts of methyl vinyl silicone rubber, 3-5 parts of rosin glycerol ester, 2-4 parts of decabromodiphenylethane, 1.5-2.5 parts of methylphenyldiethoxysilane, 0.8-1.5 parts of 1,2-dibenzoyl peroxide, 5-8 parts of nano powder, 0.8-1.6 parts of initiator, 6-9 parts of compound flame retardant, 4-7 parts of cross-linking agent and 25-30 parts of reinforcing agent.
[0009] Furthermore, the preparation method of the composite flame retardant is:
[0010] Step 1, add 20-30% of 3-aminopropyltrimethoxysilane and 15-25% of γ-glycidyloxypropyltrimethoxysilane by volume to a 70-80wt% ethanol aqueous solution, mix and stir evenly, heat it to 50-60°C, and hydrolyze it at this temperature for 2-3h; after the hydrolysis is completed, add 20-30% of inorganic powder by mass to the obtained dispersion, mix and stir evenly, heat it to 60-70°C, and keep it at this temperature for 5-8h, after the reaction is completed, filter, wash and dry the resultant components, and store the obtained pre-treated inorganic powder for standby use;
[0011] Step 2: Disperse the pretreated inorganic powder uniformly in an N,N-dimethylformamide aqueous solution with a volume concentration of 60-75% at a solid-liquid ratio of 0.03-0.08 g / mL, and then add the first flame retardant compound with a mass of 0.4-0.6 times that of the pretreated inorganic powder and the second flame retardant compound with a mass of 0.3-0.5 times that of the pretreated inorganic powder in turn, and add N,N-dimethylaniline with a mass of 3-8% of the pretreated inorganic powder after mixing and stirring evenly, and keep stirring and reacting at a temperature of 60-80°C for 15-25 hours; after the reaction is completed, filter, wash and dry the resulting components in turn, and the final result is a composite flame retardant.
[0012] Furthermore, the preparation method of the first flame retardant compound is: diphenylphosphine oxide is added to anhydrous ethanol at a dosage ratio of 0.5 to 1.0 mol / L, and 3,7-dimethyl-2,6-octadiene-1-aldehyde with a molar amount of 0.8 to 1.2 times that of diphenylphosphine oxide is added thereto, and the temperature is adjusted to 1 to 4°C after mixing and stirring evenly, and then potassium carbonate with a molar amount of 1.0 to 1.5 times that of 3,7-dimethyl-2,6-octadiene-1-aldehyde is added, and the mixture is mixed and stirred evenly, and the temperature is raised to 60 to 70°C, and the mixture is kept warm for reaction at this temperature for 5 to 8 hours; after the reaction is completed, the product components are first extracted with dichloromethane, and then washed with hydrochloric acid and deionized water in sequence to obtain the first flame retardant compound.
[0013] Furthermore, the preparation method of the inorganic powder is: add kaolin with a mass of 0.3 to 0.5 times that of magnesium chloride and a particle size of 5 to 10 μm to a magnesium chloride aqueous solution with a concentration of 0.5 to 1.0 mol / L, mix and stir evenly, adjust the pH of the resulting mixed solution to 9 to 12 with ammonia water, and keep the mixture at a temperature of 30 to 50° C. for 8 to 15 hours; after the reaction is completed, centrifuge, wash and vacuum dry the resulting product components in turn, and the final product is an inorganic powder.
[0014] Furthermore, the cross-linking agent is selected from any one of diethyl sulfide and diisopropyl sulfide.
[0015] Furthermore, the nano powder is compounded by nano alumina and nano zirconium oxide in a mass ratio of 0.5 to 0.8:1.
[0016] Furthermore, the reinforcing agent is selected from any one of fumed silica and precipitated silica.
[0017] Furthermore, the average molar mass of the methyl vinyl silicone rubber is 500,000 to 900,000 g / mol, and the molar fraction of vinyl groups therein is 0.05 to 0.2%.
[0018] Furthermore, the initiator is selected from any one of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide and 2-hydroxy-2-methyl-1-phenyl-1-propanone.
[0019] Furthermore, the preparation method of the second flame retardant compound is as follows: add 1.5 to 2.0 times the mass of cis-propylene phosphonic acid as that of carbonamide to a 20 to 30 wt % aqueous solution of carbonamide, stir and mix evenly, then raise the temperature to 80 to 95° C. in a nitrogen atmosphere, and stir and react at this temperature for 3 to 5 hours; after the reaction is completed, evaporate the water in the product; then add 2 to 4 times the mass of deionized water, 0.2 to 0.4 times the mass of hydroxypropyl deacetylated chitosan, and 0.1 to 0.15 times the mass of cyanoguanidine to the remaining mixed liquid in sequence, mix evenly, and react at a temperature of 65 to 80° C. for 3 to 6 hours; after the reaction is completed, the result is the second flame retardant compound.
[0020] Compared with the prior art, the present invention has the following beneficial effects:
[0021] In the present invention, kaolin is put into a magnesium chloride aqueous solution, and the surface of the kaolin is coated with nano magnesium hydroxide by adjusting the pH value, so as to prepare an inorganic powder with kaolin as the core and magnesium hydroxide as the shell. The obtained inorganic powder is put into a dispersion formed by hydrolyzing 3-aminopropyl trimethoxysilane and γ-glycidyloxypropyl trimethoxysilane, and the 3-aminopropyl trimethoxysilane and γ-glycidyloxypropyl trimethoxysilane react chemically with the inorganic powder through heat preservation reaction, so as to bond with the inorganic powder, and obtain a pre-treated inorganic powder.
[0022] Furthermore, the present invention puts diphenylphosphine oxide into anhydrous ethanol and adds 3,7-dimethyl-2,6-octadiene-1-aldehyde and potassium carbonate thereto, and obtains a first flame retardant compound after heat preservation reaction. Cis-propylene phosphonic acid is put into a carbonamide aqueous solution, and the mixture is stirred and reacted under the protection of a nitrogen atmosphere, and after the reaction is completed, the water in the product is evaporated, and then deionized water, hydroxypropyl deacetylated chitosan and cyanoguanidine are added to the remaining mixed liquid in sequence, and the second flame retardant compound is obtained after heat preservation reaction.
[0023] The obtained pre-treated inorganic powder is uniformly dispersed in an N,N-dimethylformamide aqueous solution, and then the first flame retardant compound and the second flame retardant compound are added thereto in sequence. The two react chemically with 3-aminopropyl trimethoxysilane and γ-glycidyl ether oxypropyl trimethoxysilane grafted on the surface of the inorganic powder under the action of N,N-dimethylaniline, and finally bonded to the surface of the inorganic powder through a chemical bond with a large force, thereby preparing a composite flame retardant. The obtained composite flame retardant has an obvious core-shell structure, the innermost layer of which is kaolin, the shell layer is magnesium hydroxide, and the outermost layer is a flame retardant layer of a three-dimensional network envelope structure composed of the first flame retardant compound and the second flame retardant compound. Under the synergistic cooperation of magnesium hydroxide and the first flame retardant compound, the flame retardant performance of the composite flame retardant is effectively guaranteed, and the ceramic silicone rubber self-adhesive material provided has excellent flame retardant and fire resistant properties. At the same time, the ceramic silicone rubber self-adhesive material provided by the present invention also has excellent bonding properties and mechanical properties, which effectively guarantees its quality. In addition, the ceramic silicone rubber self-adhesive material provided by the present invention is also convenient and quick to operate when used to repair wires and cable products. It only needs to be bonded to the damaged part at room temperature so that the two are bonded. By making it completely cover the damaged part, good insulation and high temperature resistance effects can be achieved. DETAILED DESCRIPTION
[0024] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0025] Example 1
[0026] A ceramic silicone rubber self-adhesive material, composed of the following raw materials in parts by weight: 85 parts of methyl vinyl silicone rubber, 3 parts of rosin glycerol ester, 2 parts of decabromodiphenylethane, 1.5 parts of methylphenyldiethoxysilane, 0.8 parts of 1,2-dibenzoyl peroxide, 5 parts of nano powder, 0.8 parts of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 6 parts of compound flame retardant, 4 parts of diethyl sulfide and 25 parts of fumed silica;
[0027] The nano powder is compounded by nano alumina and nano zirconium oxide in a mass ratio of 0.5:1.
[0028] The average molar mass of the methyl vinyl silicone rubber is 500000 g / mol, and the molar fraction of vinyl groups therein is 0.05%.
[0029] The preparation method of the compound flame retardant is:
[0030] Step 1, add 20% of 3-aminopropyltrimethoxysilane and 15% of γ-glycidyloxypropyltrimethoxysilane by volume to a 70wt% ethanol aqueous solution, mix and stir evenly, then heat it to 50°C, and hydrolyze it at this temperature for 2h; after the hydrolysis is completed, add 20% of inorganic powder by mass to the obtained dispersion, mix and stir evenly, then heat it to 60°C, and keep it at this temperature for 5h, after the reaction is completed, filter, wash and dry the resultant components, and store the obtained pre-treated inorganic powder for standby use;
[0031] Step 2: Disperse the pretreated inorganic powder evenly in an N,N-dimethylformamide aqueous solution with a volume concentration of 60% at a solid-liquid ratio of 0.03 g / mL, and then add the first flame retardant compound with a mass of 0.4 times that of the pretreated inorganic powder and the second flame retardant compound with a mass of 0.3 times that of the pretreated inorganic powder in turn. After mixing and stirring evenly, add N,N-dimethylaniline with a mass of 3% of the pretreated inorganic powder, and stir and react at a temperature of 60°C for 15 hours; after the reaction is completed, filter, wash and dry the resulting components in turn, and the final result is a composite flame retardant.
[0032] The preparation method of the first flame retardant compound is as follows: diphenylphosphine oxide is added into anhydrous ethanol at a dosage ratio of 0.5 mol / L, and 3,7-dimethyl-2,6-octadiene-1-aldehyde whose molar amount is 0.8 times that of diphenylphosphine oxide is added thereto, and the mixture is mixed and stirred evenly, and the temperature is adjusted to 1°C, and then potassium carbonate in an amount equal to the molar amount of 3,7-dimethyl-2,6-octadiene-1-aldehyde is added, and the mixture is mixed and stirred evenly, and the temperature is raised to 80°C, and the mixture is kept at this temperature for reaction for 5 hours; after the reaction is completed, the product components are firstly extracted with dichloromethane, and then washed with hydrochloric acid and deionized water in sequence to obtain the first flame retardant compound.
[0033] The preparation method of the inorganic powder is as follows: add kaolin with a mass 0.3 times that of magnesium chloride and a particle size of 5 μm to a magnesium chloride aqueous solution with a concentration of 0.5 mol / L, mix and stir evenly, adjust the pH of the obtained mixed solution to 9 with ammonia water, and keep the mixture at 30°C for 8 hours; after the reaction is completed, centrifuge, wash and vacuum dry the obtained product components in turn, and the final product is the inorganic powder.
[0034] The preparation method of the second flame retardant compound is as follows: add 1.5 times the mass of cis-acrylic acid of carbonamide to a 20wt% carbonamide aqueous solution, stir and mix evenly, then raise the temperature to 80°C under a nitrogen atmosphere, and stir and react at this temperature for 3 hours; after the reaction is completed, evaporate the water in the product; then add 2 times the mass of deionized water, 0.2 times the mass of hydroxypropyl deacetylated chitosan, and 0.1 times the mass of cyanoguanidine to the remaining mixed liquid in sequence, mix evenly, and react at 65°C for 3 hours; after the reaction is completed, the result is the second flame retardant compound.
[0035] Example 2
[0036] A ceramic silicone rubber self-adhesive material, composed of the following raw materials in parts by weight: 90 parts of methyl vinyl silicone rubber, 4 parts of rosin glycerol ester, 3 parts of decabromodiphenylethane, 2.0 parts of methylphenyldiethoxysilane, 1.2 parts of 1,2-dibenzoyl peroxide, 6 parts of nano powder, 1.2 parts of 2-hydroxy-2-methyl-1-phenyl-1-propanone, 8 parts of compound flame retardant, 5 parts of diisopropyl sulfide and 30 parts of precipitated silica;
[0037] The nano powder is compounded by nano alumina and nano zirconium oxide in a mass ratio of 0.6:1.
[0038] The average molar mass of the methyl vinyl silicone rubber is 700000 g / mol, and the molar fraction of vinyl groups therein is 0.15%.
[0039] The preparation method of the compound flame retardant is:
[0040] Step 1, add 25% of 3-aminopropyltrimethoxysilane and 20% of γ-glycidyloxypropyltrimethoxysilane by volume to a 75wt% ethanol aqueous solution, mix and stir evenly, then heat it to 55°C, and hydrolyze it at this temperature for 2.5h; after the hydrolysis is completed, add 25% of inorganic powder by mass to the obtained dispersion, mix and stir evenly, then heat it to 65°C, and keep it at this temperature for 6h, after the reaction is completed, filter, wash and dry the resultant components, and store the obtained pre-treated inorganic powder for standby use;
[0041] Step 2: Disperse the pretreated inorganic powder evenly in an N,N-dimethylformamide aqueous solution with a volume concentration of 70% at a solid-liquid ratio of 0.05 g / mL, and then add the first flame retardant compound with a mass of 0.5 times that of the pretreated inorganic powder and the second flame retardant compound with a mass of 0.4 times that of the pretreated inorganic powder in turn. After mixing and stirring evenly, add N,N-dimethylaniline with a mass of 5% of the pretreated inorganic powder, and stir and react at a temperature of 70°C for 20 hours; after the reaction is completed, filter, wash and dry the resulting components in turn, and the final result is a composite flame retardant.
[0042] The preparation method of the first flame retardant compound is as follows: diphenylphosphine oxide is added into anhydrous ethanol at a dosage ratio of 0.8 mol / L, and 3,7-dimethyl-2,6-octadiene-1-aldehyde in an equal molar amount to diphenylphosphine oxide is added thereto, the mixture is mixed and stirred evenly, the temperature is adjusted to 2°C, and then potassium carbonate in an amount 1.2 times that of 3,7-dimethyl-2,6-octadiene-1-aldehyde is added, the mixture is mixed and stirred evenly, the temperature is raised to 65°C, and the mixture is kept at this temperature for reaction for 6 hours; after the reaction is completed, the resultant components are first extracted with dichloromethane, and then washed with hydrochloric acid and deionized water in sequence to obtain the first flame retardant compound.
[0043] The preparation method of the inorganic powder is as follows: add kaolin with a mass 0.4 times that of magnesium chloride and a particle size of 8 μm to a magnesium chloride aqueous solution with a concentration of 0.8 mol / L, mix and stir evenly, adjust the pH of the obtained mixed solution to 10 with ammonia water, and keep the mixture at a temperature of 40°C for 12 hours; after the reaction is completed, centrifuge, wash and vacuum dry the obtained product components in turn, and the final product is the inorganic powder.
[0044] The preparation method of the second flame retardant compound is as follows: add 2.0 times the mass of cis-acrylic acid of carbonamide to a 25wt% carbonamide aqueous solution, stir and mix evenly, then raise the temperature to 90°C under a nitrogen atmosphere, and stir and react at this temperature for 4 hours; after the reaction is completed, evaporate the water in the product; then add 3 times the mass of deionized water, 0.3 times the mass of hydroxypropyl deacetylated chitosan, and 0.12 times the mass of cyanoguanidine to the remaining mixed liquid in sequence, mix evenly, and react at 75°C for 5 hours; after the reaction is completed, the result is the second flame retardant compound.
[0045] Example 3
[0046] A ceramic silicone rubber self-adhesive material, composed of the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 5 parts of rosin glycerol ester, 4 parts of decabromodiphenylethane, 2.5 parts of methylphenyldiethoxysilane, 1.5 parts of 1,2-dibenzoyl peroxide, 8 parts of nano powder, 1.6 parts of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 9 parts of compound flame retardant, 7 parts of diethyl sulfide and 30 parts of fumed silica;
[0047] The nano powder is compounded by nano alumina and nano zirconium oxide in a mass ratio of 0.8:1.
[0048] The average molar mass of the methyl vinyl silicone rubber is 900000 g / mol, and the molar fraction of vinyl groups therein is 0.2%.
[0049] The preparation method of the compound flame retardant is:
[0050] Step 1, add 30% of 3-aminopropyltrimethoxysilane and 25% of γ-glycidyloxypropyltrimethoxysilane by volume to 80wt% ethanol aqueous solution, mix and stir evenly, then heat it to 60°C, and hydrolyze it at this temperature for 3h; after the hydrolysis is completed, add 30% of inorganic powder by mass to the obtained dispersion, mix and stir evenly, then heat it to 70°C, and keep it at this temperature for 8h, after the reaction is completed, filter, wash and dry the resultant components, and store the obtained pre-treated inorganic powder for standby use;
[0051] Step 2: Disperse the pretreated inorganic powder evenly in an N,N-dimethylformamide aqueous solution with a volume concentration of 75% at a solid-liquid ratio of 0.08 g / mL, and then add the first flame retardant compound with a mass of 0.6 times that of the pretreated inorganic powder and the second flame retardant compound with a mass of 0.5 times that of the pretreated inorganic powder in turn. After mixing and stirring evenly, add N,N-dimethylaniline with a mass of 8% of the pretreated inorganic powder, and stir and react at 80°C for 25 hours; after the reaction is completed, filter, wash and dry the resulting components in turn, and the final result is a composite flame retardant.
[0052] The preparation method of the first flame retardant compound is as follows: diphenylphosphine oxide is added into anhydrous ethanol at a dosage ratio of 1.0 mol / L, and 3,7-dimethyl-2,6-octadiene-1-aldehyde whose molar amount is 1.2 times that of diphenylphosphine oxide is added thereto, and the temperature is adjusted to 4°C after mixing and stirring evenly, and then potassium carbonate whose molar amount is 1.5 times that of 3,7-dimethyl-2,6-octadiene-1-aldehyde is added, and the temperature is raised to 70°C after mixing and stirring evenly, and the reaction is kept at this temperature for 8 hours; after the reaction is completed, the product components are firstly extracted with dichloromethane, and then washed with hydrochloric acid and deionized water in sequence to obtain the first flame retardant compound.
[0053] The preparation method of the inorganic powder is as follows: add kaolin with a mass 0.5 times that of magnesium chloride and a particle size of 10 μm to a magnesium chloride aqueous solution with a concentration of 1.0 mol / L, mix and stir evenly, adjust the pH of the obtained mixed solution to 12 with ammonia water, and keep the mixture at a temperature of 50°C for 15 hours; after the reaction is completed, centrifuge, wash and vacuum dry the obtained product components in turn, and the final product is the inorganic powder.
[0054] The preparation method of the second flame retardant compound is as follows: add 2.0 times the mass of cis-acrylic acid of carbonamide to a 30wt% carbonamide aqueous solution, stir and mix evenly, then raise the temperature to 95°C under a nitrogen atmosphere, and stir and react at this temperature for 5 hours; after the reaction is completed, evaporate the water in the product; then add 4 times the mass of deionized water, 0.4 times the mass of hydroxypropyl deacetylated chitosan, and 0.15 times the mass of cyanoguanidine to the remaining mixed liquid in sequence, mix evenly, and react at 80°C for 6 hours; after the reaction is completed, the result is the second flame retardant compound.
[0055] Comparative Example 1: The main difference between this example and Example 1 is that this example uses an equal amount of kaolin instead of the compound flame retardant.
[0056] Comparative Example 2: The main difference between this example and Example 1 is that this example uses an equal amount of inorganic powder to replace the compound flame retardant.
[0057] Comparative Example 3: The main difference between this example and Example 1 is that an equal amount of the first flame retardant compound is used to replace the second flame retardant compound.
[0058] Comparative Example 4: The main difference between this embodiment and embodiment 1 is that an equal amount of a second flame retardant compound is used to replace the first flame retardant compound; and the total amount of the second flame retardant compound in this embodiment is equal to the first flame retardant compound in Comparative Example 3.
[0059] Performance Testing
[0060] The relevant properties of the ceramic silicone rubber self-adhesive materials provided in Examples 1 to 3 and Comparative Examples 1 to 4 were tested respectively, and the obtained test data were recorded in the following table:
[0061]
[0062] By comparing and analyzing the relevant data in the table, it can be seen that the ceramic silicone rubber self-adhesive material provided by the present invention not only has excellent bonding properties and mechanical properties, but also has excellent flame retardant properties, which effectively guarantees the quality of the ceramic silicone rubber self-adhesive material. This shows that the ceramic silicone rubber self-adhesive material provided by the present invention has a broader market prospect and is more suitable for promotion.
[0063] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0064] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A ceramic silicone rubber self-adhesive material, characterized in that: The invention is composed of the following raw materials in parts by weight: 85 to 100 parts of methyl vinyl silicone rubber, 3 to 5 parts of rosin glycerol ester, 2 to 4 parts of decabromodiphenylethane, 1.5 to 2.5 parts of methylphenyldiethoxysilane, 0.8 to 1.5 parts of 1,2-dibenzoyl peroxide, 5 to 8 parts of nano powder, 0.8 to 1.6 parts of initiator, 6 to 9 parts of compound flame retardant, 4 to 7 parts of crosslinking agent and 25 to 30 parts of reinforcing agent; The composite flame retardant is prepared by the following method: The kaolin is put into a magnesium chloride aqueous solution, and the surface of the kaolin is coated with nano-magnesium hydroxide by adjusting the pH value, so as to prepare an inorganic powder with kaolin as the core and magnesium hydroxide as the shell; the obtained inorganic powder is put into a dispersion formed by hydrolyzing 3-aminopropyltrimethoxysilane and γ-glycidyloxypropyltrimethoxysilane, and the pre-treated inorganic powder is obtained by heat preservation reaction; Putting diphenylphosphine oxide into anhydrous ethanol and adding 3,7-dimethyl-2,6-octadiene-1-aldehyde and potassium carbonate thereto, and reacting at a temperature of 1 000 ℃ to obtain a first flame retardant compound; putting cis-propylenephosphonic acid into a carbonamide aqueous solution, and reacting at a temperature of 1 000 ℃ under the protection of a nitrogen atmosphere with stirring, and after the reaction is completed, evaporating the water in the product, and then adding deionized water, hydroxypropyl deacetylated chitosan and cyanoguanidine to the remaining mixed liquid in sequence, and reacting at a temperature of 1 000 ℃ to obtain a second flame retardant compound; The obtained pre-treated inorganic powder is uniformly dispersed in an N,N-dimethylformamide aqueous solution, and then a first flame retardant compound and a second flame retardant compound are sequentially added thereto, and the two react chemically with 3-aminopropyltrimethoxysilane and γ-glycidyloxypropyltrimethoxysilane grafted on the surface of the inorganic powder under the action of N,N-dimethylaniline, thereby preparing a composite flame retardant; The reinforcing agent is selected from any one of fumed silica and precipitated silica.
2. A ceramic silicone rubber self-adhesive material according to claim 1, characterized in that: The preparation method of the composite flame retardant is: Step 1, add 20-30% of 3-aminopropyltrimethoxysilane and 15-25% of γ-glycidyloxypropyltrimethoxysilane by volume to a 70-80wt% ethanol aqueous solution, mix and stir evenly, heat it to 50-60°C, and hydrolyze it at this temperature for 2-3h; after the hydrolysis is completed, add 20-30% of inorganic powder by mass to the obtained dispersion, mix and stir evenly, heat it to 60-70°C, and keep it at this temperature for 5-8h, after the reaction is completed, filter, wash and dry the resultant components, and store the obtained pre-treated inorganic powder for standby use; Step 2: Disperse the pretreated inorganic powder uniformly in an N,N-dimethylformamide aqueous solution with a volume concentration of 60-75% at a solid-liquid ratio of 0.03-0.08 g / mL, and then add the first flame retardant compound with a mass of 0.4-0.6 times that of the pretreated inorganic powder and the second flame retardant compound with a mass of 0.3-0.5 times that of the pretreated inorganic powder in turn, and add N,N-dimethylaniline with a mass of 3-8% of the pretreated inorganic powder after mixing and stirring evenly, and keep stirring and reacting at a temperature of 60-80°C for 15-25 hours; after the reaction is completed, filter, wash and dry the resulting components in turn, and the final result is a composite flame retardant.
3. A ceramic silicone rubber self-adhesive material according to claim 2, characterized in that: The preparation method of the first flame retardant compound is as follows: diphenylphosphine oxide is added into anhydrous ethanol at a dosage ratio of 0.5 to 1.0 mol / L, and 3,7-dimethyl-2,6-octadiene-1-aldehyde whose molar amount is 0.8 to 1.2 times of diphenylphosphine oxide is added thereto, and the temperature is adjusted to 1 to 4°C after mixing and stirring evenly, and then potassium carbonate whose molar amount is 1.0 to 1.5 times of 3,7-dimethyl-2,6-octadiene-1-aldehyde is added, and the temperature is raised to 60 to 70°C after mixing and stirring evenly, and the reaction is kept at this temperature for 5 to 8 hours; after the reaction is completed, the product components are firstly extracted with dichloromethane, and then washed with hydrochloric acid and deionized water in sequence to obtain the first flame retardant compound.
4. A ceramic silicone rubber self-adhesive material according to claim 2, characterized in that: The preparation method of the inorganic powder is as follows: adding kaolin with a mass of 0.3 to 0.5 times that of magnesium chloride and a particle size of 5 to 10 μm to a magnesium chloride aqueous solution with a concentration of 0.5 to 1.0 mol / L, mixing and stirring evenly, adjusting the pH of the obtained mixed solution to 9 to 12 with ammonia water, and keeping the mixture at a temperature of 30 to 50° C. for 8 to 15 hours; after the reaction is completed, centrifuging, washing and vacuum drying the obtained product components in sequence, and finally obtaining the inorganic powder.
5. The ceramic silicone rubber self-adhesive material according to claim 1, characterized in that: The cross-linking agent is selected from any one of diethyl sulfide and diisopropyl sulfide.
6. The ceramic silicone rubber self-adhesive material according to claim 1, characterized in that: The nanometer powder is compounded by nanometer aluminum oxide and nanometer zirconium oxide in a mass ratio of 0.5 to 0.8:
1.
7. The ceramic silicone rubber self-adhesive material according to claim 1, characterized in that: The average molar mass of the methyl vinyl silicone rubber is 500,000 to 900,000 g / mol, and the molar fraction of vinyl groups therein is 0.05 to 0.2%.
8. The ceramic silicone rubber self-adhesive material according to claim 1, characterized in that: The initiator is selected from any one of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide and 2-hydroxy-2-methyl-1-phenyl-1-propanone.
9. The ceramic silicone rubber self-adhesive material according to claim 2, characterized in that: The preparation method of the second flame retardant compound is as follows: add 1.5 to 2.0 times the mass of cis-propylenephosphonic acid in a 20 to 30 wt% aqueous solution of carbonamide to the mixture, stir well and then raise the temperature to 80 to 95°C in a nitrogen atmosphere, and stir and react at this temperature for 3 to 5 hours; after the reaction is completed, evaporate the water in the product; then add 2 to 4 times the mass of deionized water, 0.2 to 0.4 times the mass of hydroxypropyl deacetylated chitosan and 0.1 to 0.15 times the mass of cyanoguanidine to the remaining mixed liquid in sequence, mix well and react at 65 to 80°C for 3 to 6 hours; after the reaction is completed, the result is the second flame retardant compound.
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